反应详情

A mixture of 5.75 g of 3-(hydroxymethyl)piperidine, 13.8 ml of triethylamine and 10 g of 2-(3,4-dimethoxyphenyl)-ethyl chloride was heated under reflux for 4 hours. After the reaction mixture had cooled, it was acidified with about 30 ml of aqueous 2N hydrochloric acid solution, and unreacted 2-(3,4-dimethoxyphenyl)-ethyl chloride was separated by extraction with tert-butyl methyl ether. The aqueous phase was then rendered alkaline by addition of sodium hydroxide solution and was extracted with dichloromethane. The organic phase was separated, dried and concentrated. 5.3 g of N-[2-(3,4-dimethoxyphenyl)-ethyl]-3-(hydroxymethyl)-piperidine were obtained.

1. temperaturewas heated
2. temperatureunder reflux for 4 hours
3. temperatureAfter the reaction mixture had cooled
4. customwas separated by extraction with tert-butyl methyl ether
5. additionby addition of sodium hydroxide solution
6. extractionwas extracted with dichloromethane
7. customThe organic phase was separated
8. customdried
9. concentrationconcentrated